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Method for preparing 10-undecylenic acid and heptanal by catalytic cracking

A technology of catalytic cracking and heptanal, applied in chemical instruments and methods, molecular sieve catalysts, preparation of carbon-based compounds, etc., can solve the problems of high viscosity, difficult gasification, and poor fluidity of castor oil, and achieve lower reaction temperature and higher yield. efficiency, reducing the effect of polymerization and isomerization reactions

Active Publication Date: 2016-06-01
江苏东鼎化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high viscosity of castor oil in this process, it has poor fluidity and is difficult to gasify, and coking is more difficult to control
[0004] The above two methods are based on the thermal cracking process. Because the thermal cracking temperature is too high, the double bond polymerization and isomerization reaction, the secondary cracking of the product, coking and other side reactions have a large ratio, and the product yield is difficult to increase.

Method used

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  • Method for preparing 10-undecylenic acid and heptanal by catalytic cracking

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preheating furnace adopts Φ30×1000mm stainless steel tube, filled with ceramic Raschig ring filler, and the cracking furnace adopts Φ40×1000mm stainless steel tube, filled with cracking catalyst I. The temperature inside the preheating furnace and the cracking furnace is automatically controlled by a temperature controller. The preheating temperature and cracking temperature are detected respectively at the outlet of the preheating furnace and the cracking furnace.

[0026] Methyl ricinoleate was added dropwise at 5.8ml / min, water was added dropwise at 6.0ml / min, mixed into the preheating furnace, heated to 250°C, introduced into the cracking furnace, catalytically cracked at 420°C, the cracked mixed gas was condensed and collected and weighed Heavy, 10-undecylenic acid methyl ester and heptanal content were analyzed by gas chromatography. The calculated yield of methyl 10-undecylenate was 46.5%, and the yield of heptanal was 25.7%.

Embodiment 2

[0028] The preheating furnace adopts Φ30×1000mm stainless steel tube, filled with ceramic Raschig ring filler, and the cracking furnace adopts Φ40×1000mm stainless steel tube, filled with cracking catalyst II. The temperature inside the preheating furnace and the cracking furnace is automatically controlled by a temperature controller. The preheating temperature and cracking temperature are detected respectively at the outlet of the preheating furnace and the cracking furnace.

[0029] Methyl ricinoleate was added dropwise at 4.5ml / min, water was added dropwise at 6.0ml / min, mixed into the preheating furnace and heated to 350°C, introduced into the cracking furnace, catalytically cracked at 480°C, the cracked mixed gas was condensed and collected and weighed Heavy, 10-undecylenic acid methyl ester and heptanal content were analyzed by gas chromatography. The calculated yield of methyl 10-undecylenate was 48.3%, and the yield of heptanal was 26.4%.

Embodiment 3

[0031] The preheating furnace adopts Φ30×1000mm stainless steel tube, filled with ceramic Raschig ring filler, and the cracking furnace adopts Φ40×1000mm stainless steel tube, filled with cracking catalyst I. The temperature inside the preheating furnace and the cracking furnace is automatically controlled by a temperature controller. The preheating temperature and cracking temperature are detected respectively at the outlet of the preheating furnace and the cracking furnace.

[0032] Methyl ricinoleate was added dropwise at 7.5ml / min, water was added dropwise at 5.0ml / min, mixed into the preheating furnace and heated to 280°C, introduced into the cracking furnace, catalytically cracked at 460°C, the cracked mixed gas was condensed and collected and weighed Heavy, 10-undecylenic acid methyl ester and heptanal content were analyzed by gas chromatography. The calculated yield of methyl 10-undecylenate was 45.8%, and the yield of heptanal was 24.2%.

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Abstract

The invention relates to a process for producing polyundecancylamide resin through castor oil and particularly relates to a method for preparing 10-undecenoic acid and heptanal through the castor oil in the process. The method comprises the following steps: ester interchange is performed on the castor oil and methyl alcohol to generate ricinic acid methyl ester; catalytic cracking is performed on the ricinic acid methyl ester to generate10-undecenoic acid methyl ester and heptanal; pressure-reduction rectification separation is performed on the 10-undecenoic acid methyl ester and heptana; saponification and acidification are performed on the 10-undecenoic acid methyl ester and heptana, so that 10-undecylenic acid is obtained; the ricinic acid methyl ester is mixed with water (or water vapor) according to the mass ratio of 1:(0.5-2), the mixture is preheated to 200-400 DEG C, and then is loaded into a cracking still filled with a catalyst, and cracking is performed at the temperature of 400-500 DEG C, so that the 10-undecenoic acid and heptanal are generated. According to the invention, due to catalytic action, the cracking temperature is reduced greatly, so that side reactions such as polymerization and isomerization of the double bond, the secondary cracking of a product and coking are reduced, and the yield of the 10-undecenoic acid and heptanal is improved greatly.

Description

technical field [0001] The invention relates to a process for producing nylon 11 resin from castor oil, in particular to a method for preparing 10-undecenoic acid and heptanal from castor oil in the process. Background technique [0002] The chemical name of nylon 11 is polyundecylactam, the English name is Polyundecancylamide (abbreviated as PA11), and the chemical structure is H[NH(CH 2 ) 10 CO] n OH, a long carbon chain soft nylon synthesized from castor oil, is an important variety of polyamide engineering plastics. The production of nylon 11 mainly includes the production of 10-undecylenic acid, 11-aminoundecylic acid, monomer polymerization and resin modification. [0003] There are two main processes for producing 10-undecylenic acid from castor oil in China: one is the traditional lead bath cracking technology, which mixes methyl ricinoleate and water vapor into high-temperature lead liquid for cracking, and the lead liquid is easy to As the pyrolysis products vo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C57/03C07C51/02C07C47/02C07C45/51B01J29/70B01J29/44
CPCB01J29/44B01J29/7034B01J2229/12B01J2229/18B01J2229/20B01J2229/24C07C45/512C07C51/02C07C67/293C07C57/03C07C69/533C07C47/02
Inventor 唐昌盛袁志红
Owner 江苏东鼎化学科技有限公司
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